CN108962415B - Method for efficiently and deeply recovering hydrogen/deuterium in hydrogen/lithium deuteride - Google Patents
Method for efficiently and deeply recovering hydrogen/deuterium in hydrogen/lithium deuteride Download PDFInfo
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- CN108962415B CN108962415B CN201710366458.2A CN201710366458A CN108962415B CN 108962415 B CN108962415 B CN 108962415B CN 201710366458 A CN201710366458 A CN 201710366458A CN 108962415 B CN108962415 B CN 108962415B
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Abstract
The invention discloses a method for efficiently and deeply recovering hydrogen/deuterium in hydrogen/lithium deuteride, which comprises the following steps: 1) preparing a reaction system; 2) checking the leakage rate of the reaction device; 3) pretreating reactants; 4) mixing the materials; 5) heating to release hydrogen; 6) and (5) post-reaction treatment. Wherein the activating agent adopted in the heating reaction step in the step 5) is porous oxide selected from one or more of mesoporous silica SBA-15, microporous silica/alumina MCM-41, MCM-22 and mesoporous titanium dioxide. The method has the advantages of simple operation, low cost, low reaction temperature, high recovery efficiency of hydrogen isotopes, small residual amount of hydrogen in products, single product composition, environmental friendliness, convenience in treatment and the like, and can be used for large-scale experiments.
Description
Technical Field
The invention belongs to the field of nuclear technology application, and particularly relates to a method for efficiently and deeply recovering hydrogen/deuterium in hydrogen/lithium deuteride.
Background
Lithium hydride (deuteride) is an important nuclear energy material and hydrogen storage (deuterium) material, and is applied to nuclear chemistry and energy industry, and the hydrogen/deuterium in the lithium hydride (deuteride) needs to be recovered under partial application scenes. However, lithium hydride (deuteride) has very high thermal stability, the decomposition temperature reaches 850 ℃, and hydrogen/deuterium in the lithium hydride (deuteride) cannot be recovered under mild conditions. Generally, an activating agent is added to activate lithium hydride (deuteride) so that the lithium hydride (deuteride) is decomposed at a lower temperature to release hydrogen/deuterium, thereby achieving the purpose of recovering hydrogen/deuterium gas therein. Two classes of materials are currently used as activators: one is a low melting point metal, and the other is an inorganic oxide such as silicon oxide. Among them, low melting point metals react with lithium hydride at around 400 ℃ to release hydrogen, but have a problem that the reaction product is an alloy of lithium, and hydrogen is easily retained in the metal, thus making it difficult to deeply recover hydrogen. Inorganic oxides such as silica are commonly used as activators for the decomposition of lithium hydride, and the reaction product has a small amount of residual hydrogen but has a high temperature (690 ℃ or higher) for complete reaction. Inorganic oxides are better candidates for deep recovery of hydrogen/deuterium from lithium hydride (deuteride) than both materials, but how to further reduce the reaction temperature and increase the recovery rate is a difficulty in this process.
Therefore, the invention provides a method for efficiently and deeply recovering hydrogen/deuterium in hydrogen/lithium deuteride. Surprisingly, the method can release hydrogen/deuterium gas from hydrogen/lithium deuteride at lower temperature, and the recovery rate of hydrogen/deuterium can reach more than 99.5%.
Disclosure of Invention
Aiming at the problems in the prior art of recovering hydrogen/deuterium from lithium hydrogen/deuteride, the invention aims to provide a method for deeply recovering hydrogen/deuterium with high efficiency at lower temperature.
The technical scheme adopted by the invention is as follows:
a method for efficiently and deeply recovering hydrogen/deuterium in hydrogen/lithium deuteride comprises the step of reacting porous oxide serving as an activating agent with the hydrogen/lithium deuteride to recover the hydrogen/deuterium.
The method for efficiently and deeply recovering hydrogen/deuterium in hydrogen/lithium deuteride comprises the steps of heating the porous oxide to 400-500 ℃, roasting for 0.5-1h, cooling, uniformly mixing with the hydrogen/lithium deuteride, heating to release hydrogen/deuterium, and recovering the hydrogen/deuterium.
The porous oxide is heated and pretreated to be beneficial to removing impurities in the porous oxide, so that the content of the impurities in the gas after reaction is reduced.
In the method for efficiently and deeply recovering hydrogen/deuterium in hydrogen/lithium deuteride, the temperature for heating the porous oxide and the hydrogen/lithium deuteride to release the hydrogen/deuterium is 300-620 ℃.
The present inventors have surprisingly found that porous oxides can lower the reaction energy barrier and thus start the reaction at a lower temperature, especially in combination with the pretreatment of the porous oxide. The method of the invention can adopt the low temperature range, the prior art method can not completely react, and at the same high temperature, the method of the invention has faster reaction and shorter time consumption, and simultaneously ensures the gas recovery rate and the gas purity, and the recovery rate is up to more than 99.5 percent.
According to the method for efficiently and deeply recovering hydrogen/deuterium in hydrogen/lithium deuteride, the porous oxide is selected from one or more of mesoporous silica SBA-15, microporous silica/alumina MCM-41, MCM-22 and mesoporous titanium dioxide, and preferably mesoporous silica.
Preferably, the porous oxide has a density of less than 1g/cm3。
The method for efficiently and deeply recovering hydrogen/deuterium in hydrogen/lithium deuteride specifically comprises the following steps:
1) design and integration of the reaction device: the reaction device comprises a vacuum pump 1, a high-purity argon device 2, a flow-through reactor 3, a pressure sensor 4, a uranium bed 5, a gas standard tank 6 and a gas chromatograph 7, and the devices are connected with one another through valves and stainless steel pipelines according to a conventional connection mode;
2) and (3) testing the leakage rate of the reaction device: evacuating the system to 2Pa through a vacuum pump 1, filling helium to 1.5MPa, and maintaining the pressure for 1 h;
3) pretreatment of materials: heating the porous oxide to 400-500 ℃, and roasting at high temperature for 0.5-1 h;
4) mixing materials: uniformly mixing the porous oxide treated and cooled in the step 3) with lithium hydride, wherein the content of the lithium hydride is 5-85 wt%;
5) heating to release hydrogen/deuterium: placing the mixture obtained in the step 4) in a flow-through reactor 3, connecting the flow-through reactor to a system, evacuating the reaction system to below 2Pa, and heating the reactor to 300-620 ℃;
6) and (3) post-reaction treatment: the hydrogen/deuterium gas volume in the gas standard tank 6 is metered and the gas composition is analysed using gas chromatography 7 and the gas is recycled to the uranium bed 5 for use.
The flow reactor 3 consists of a stainless steel outer casing, a dust filter, a heater and a temperature thermocouple, and the bed body is sealed by adopting a flange structure. The uranium bed 5 comprises outer covering shell, dust filter, heater and temperature thermocouple, and the bed body adopts the full seal to weld the structure, encapsulates the uranium granule in the bed, and the granularity is 20 ~ 80 meshes for absorb the hydrogen isotope gas that the reaction produced. Gaseous standard jar 6 is 2L's cylindric stainless steel container for a volume for carry out the gaseous temporary storage of hydrogen isotope and volume measurement, and the device moves, and standard jar one end and pressure sensor intercommunication, accessible pressure sensor real-time observation jar internal pressure variation condition, pressure sensor 4 record gaseous pressure, when pressure numerical value no longer changes, think the reaction and end. The high purity argon gas device 2 is used for providing carrier gas for the gas chromatograph 7 and purging the system. These devices are all available from conventional commercial sources.
According to some embodiments of the present invention, the above step 2) is performed by examining the leak rate of the reaction device, and the leak rate is less than 1.0 × 10-9·Pa·m3·s-1。
According to some embodiments of the present invention, the step 3) is performed by baking under air, nitrogen, argon atmosphere or vacuum, preferably in air.
The method for efficiently and deeply recovering hydrogen/deuterium in hydrogen/lithium deuteride comprises the step 3) of crushing the porous oxide to 1nm-50 mu m.
According to the method for efficiently and deeply recovering hydrogen/deuterium in hydrogen/lithium deuteride, the materials in the step 4) can be mixed and then can be in a powder form or a tablet. Some embodiments of the invention pack the mixture into a sheet form and then feed into a reactor.
As a preferred technical scheme, the content of hydrogen/lithium deuteride in the mixed material in the step (4) is 20-40 wt.%. The reaction effect and the recovery efficiency can be simultaneously considered under the content proportion.
As a preferable technical scheme, in the step (4), hydrogen/deuterium is heated, and the reactor is heated to 400-610 ℃.
The method for efficiently and deeply recovering hydrogen/deuterium in hydrogen/lithium deuteride provided by the invention has the advantages that the porous oxide is reasonably utilized, the specific surface area of a reactant is increased, the particle size of the reactant is reduced, and the reaction energy barrier is obviously reduced, so that the effect of reducing the reaction temperature is achieved, lithium hydride releases hydrogen at a lower temperature, the initial temperature of the reaction temperature can even be as low as 300 ℃, the reaction hardly occurs at the temperature in the prior art, the reaction needs to be started at the temperature of more than 510 ℃, and the improvement effect has obvious advantages in multiple aspects such as energy consumption, safety, cost and the like. Specifically, the method of the present invention has the following beneficial effects:
1) the method is simple to operate, low in cost and applicable to large-scale experiments;
2) the density of the porous oxide used in the method is equivalent to that of lithium hydride (deuteride), and the porous oxide has large specific surface area, higher reaction activity, low reaction temperature and high recovery efficiency of hydrogen/deuterium;
3) the product of the method has the advantages of small residual quantity of hydrogen/deuterium, single composition, environmental protection and convenient treatment.
Drawings
FIG. 1 is a schematic diagram of an apparatus for deep recovery of hydrogen/deuterium from lithium hydrogen/deuteride according to the present invention; the device comprises a vacuum pump 1, a high-purity argon device 2, a flow-through reactor 3, a pressure sensor 4, a uranium bed 5, a gas standard tank 6 and a gas chromatograph 7, wherein the devices are connected with a stainless steel pipeline by valves according to the figure;
FIG. 2 is an XRD spectrum of the feed mixture of example 1 of the present invention;
FIG. 3 is an XRD spectrum of a reaction product in example 1 of the present invention;
FIG. 4 is a graph showing the relationship between the pressure of deuterium released from the raw material and the reaction temperature in the deuterium releasing process in example 1 of the present invention;
1 is a temperature-time change curve, 2 is a deuterium pressure-time change curve, the mixture starts to react at about 300 ℃, the deuterium release amount increases (the deuterium pressure increases) along with the increase of the temperature, the reaction rate is high, and the reaction is nearly completed when the reaction reaches about 600 ℃.
Detailed Description
The following are only some preferred embodiments of the present invention, and it should not be understood that the scope of the above-described subject matter of the present invention is limited to the following examples. All the technologies implemented based on the above-mentioned contents of the present invention belong to the protection scope of the present invention.
Example 1
Referring to the installation device of FIG. 1, the system is evacuated to 2Pa, filled with He to 1.5MPa and kept for 1h, and leakage detection is carried out until the leakage rate is less than 1.0 multiplied by 10-9·Pa·m3·s-1And then is ready for use. Mixing mesoporous silica SBA-15 (density less than 1 g/cm)3) Heating to 500 deg.C in air atmosphere, calcining at high temperature for 0.5 hr, and pulverizing to 100nm or less. Mixing the calcined mesoporous silica SBA-15 with lithium deuteride according to the weight ratio of 64: 36 weight ratio, pressing the mixture into a sheet shape under the protection of nitrogen and 25MPa pressure, and loading the sheet into a reactor. The reactor is connected to the system, the system is vacuumized to be below 2Pa, and the lithium deuteride is heated to 300 ℃ to start to decompose and release deuterium gas. The decomposed deuterium gas was stored in a gas standard tank and the pressure of the gas was recorded using a pressure sensor until the pressure no longer changed (600 ℃), and the reaction was considered complete. The composition of the gas was analysed by chromatography and the gas was collected in a uranium bed for use. The composition of the collected gas is shown in table 1, and the recovered deuterium gas is very pure. XRD of the reaction feed mixture and product are shown in figures 2 and 3, respectively, with deuterium recovery of greater than 99.5% calculated by theory. FIG. 4 is a graph of the pressure of deuterium released during the release of deuterium from the starting material versus reaction temperature.
TABLE 1 gas composition and content after reaction
| Gas component | D2 | O2 | N2 | CH4 | CO |
| Content (wt.) | 99.95％ | <30ppm | <30ppm | <50ppm | <50ppm |
Using the same apparatus, the reaction was carried out in a conventional manner using conventional spherical silica as an activator, and the reaction could not be carried out at the above-mentioned temperature. The initial reaction temperature was 510 ℃ and at 600 ℃ the reaction was still incomplete. Under the same conditions, the recovery rate of deuterium in the system using spherical silica as an activator is only 60% at 600 ℃.
Example 2
Evacuating the system to 2Pa, filling He to 1.5MPa, and maintaining the pressure for 1h, wherein the leakage rate is less than 1.0 × 10-9·Pa·m3·s-1And then is ready for use. Microporous silica/alumina MCM-41 (density less than 1 g/cm)3) Heating to 450 deg.C in air atmosphere, calcining at high temperature for 0.5 hr, and pulverizing to 100nm or less. The calcined microporous silica/alumina MCM-41 was mixed with lithium deuteride according to a 79: 21 weight ratio, pressing the mixture into sheets under the protection of nitrogen and 25MPa pressure, and loading into the reactor. The reactor is connected to the system, the system is vacuumized to be below 2Pa, the temperature is heated to be above 350 ℃, and lithium deuteride begins to decompose to release deuterium gas. The decomposed deuterium gas was stored in a gas standard tank and the pressure of the gas was recorded using a pressure sensor until the pressure no longer changed (600 ℃), and the reaction was considered complete. The composition of the gas was analysed by chromatography and the gas was collected in a uranium bed for use. The composition of the collected gases is shown in table 2, and the recovered deuterium gas is very pure with a deuterium recovery rate of > 99.5% calculated by theory.
TABLE 2 gas composition and content after reaction
| Gas component | D2 | O2 | N2 | CH4 | CO |
| Content (wt.) | 99.95％ | <30ppm | <30ppm | <50ppm | <50ppm |
Using the same apparatus, deuterium releasing reaction was carried out at the same reaction temperature and by the conventional method using the conventional spherical silica as an activator, and the method of this example was carried out at a lower initial reaction temperature and a higher reaction rate, and the recovery rate of deuterium was 60% in the system using the spherical silica as an activator at 600 ℃.
Example 3
Evacuating the system to 2Pa, filling He to 1.5MPa, and maintaining the pressure for 1h, wherein the leakage rate is less than 1.0 × 10-9·Pa·m3·s-1And then is ready for use. Mixing mesoporous silica SBA-15 (density less than 1 g/cm)3) Heating to 500 deg.C in air atmosphere, calcining at high temperature for 0.5 hr, and pulverizing to powder of 100nm or less. And (3) mixing the calcined mesoporous silica SBA-15 lithium hydride according to the weight ratio of 60: 40 parts by weight, pressing the mixture into a sheet shape under the protection of nitrogen and 25MPa, and loading the sheet into a reactor. The reactor is connected to a system, the system is vacuumized to be below 2Pa, the temperature is heated to be above 330 ℃, and lithium hydride begins to decompose to release hydrogen. The decomposed hydrogen was stored in a gas standard tank and the pressure of the gas was recorded using a pressure sensor until the pressure no longer changed (610 ℃), and the reaction was considered complete. The composition of the gas was analysed by chromatography and the gas was collected in a uranium bed for use. The composition of the collected gas is shown in table 3, and the recovered hydrogen is very pure with a hydrogen recovery of > 99.5% calculated as theoretical.
TABLE 3 gas composition and content after reaction
| Gas component | H2 | O2 | N2 | CH4 | CO |
| Content (wt.) | 99.95％ | <30ppm | <30ppm | <50ppm | <50ppm |
The hydrogen release reaction is carried out by using the same device and using the conventional spherical silica as an activating agent according to a conventional method at the same reaction temperature, the initial reaction temperature of the method is lower, the reaction rate is high, and the system hydrogen recovery rate of the spherical silica as the activating agent is 57% at 610 ℃.
Claims (11)
1. A method for highly efficiently and deeply recovering hydrogen/deuterium in hydrogen/lithium deuteride is characterized by comprising the steps of reacting porous oxide serving as an activating agent with the hydrogen/lithium deuteride and recovering the hydrogen/deuterium, wherein the porous oxide is adopted to reduce the reaction energy barrier so as to reduce the reaction temperature;
the porous oxide is selected from one or more of mesoporous silica SBA-15, microporous silica/alumina MCM-41, MCM-22 and mesoporous titanium dioxide.
2. The method as claimed in claim 1, wherein the porous oxide is heated to 400-500 ℃, baked for 0.5-1h, cooled and uniformly mixed with the lithium hydride/deuteride, and heated to release/deuterium, thereby recovering hydrogen/deuterium.
3. The method as claimed in claim 1, wherein the porous oxide and the lithium hydride/deuteride are heated to release hydrogen/deuterium at a temperature of 300-620 ℃.
4. The method for efficient deep recovery of hydrogen/deuterium from lithium hydrogen/deuteride according to claim 1, wherein the density of said porous oxide is less than 1g/cm3。
5. The method for highly efficient deep recovery of hydrogen/deuterium from lithium hydrogen/deuteride as claimed in claim 1, comprising the steps of:
1) design and integration of the reaction device: the reaction device comprises a vacuum pump (1), a high-purity argon device (2), a flow-through reactor (3), a pressure sensor (4), a uranium bed (5), a gas standard tank (6) and a gas chromatograph (7), and the devices are connected with each other through a valve and a stainless steel pipeline according to a conventional connection mode;
2) and (3) testing the leakage rate of the reaction device: evacuating the system to 2Pa through a vacuum pump (1), filling helium to 1.5MPa, and maintaining the pressure for 1 h;
3) pretreatment of materials: heating the porous oxide to 400-500 ℃, and roasting at high temperature for 0.5-1 h;
4) mixing materials: uniformly mixing the porous oxide treated and cooled in the step 3) with hydrogen/lithium deuteride, wherein the content of the hydrogen/lithium deuteride is 5-85 wt%;
5) heating to release hydrogen/deuterium: placing the mixture obtained in the step 4) into a flow-through reactor 3) and connecting the mixture into a system, evacuating the reaction system to below 2Pa, and heating the reactor to 300-620 ℃;
6) and (3) post-reaction treatment: the volume of hydrogen/deuterium gas in the gas standard tank (6) is measured and the gas composition is analysed by gas chromatography (7) and the gas is recycled to the uranium bed (5) for use.
6. The method as claimed in claim 5, wherein the leak rate of the reaction apparatus in step 2) is less than 1.0 x 10 by testing the leak rate of the reaction apparatus-9·Pa·m3·s-1。
7. The method for highly efficient deep recovery of hydrogen/deuterium in hydrogen/lithium deuteride as claimed in claim 5, wherein the step 3) is performed by calcining under air, nitrogen, argon atmosphere or vacuum condition.
8. The method for the efficient deep recovery of hydrogen/deuterium in hydrogen/lithium deuteride according to claim 5, wherein step 3) further comprises pulverizing the porous oxide to 1nm-50 um.
9. The method for highly efficient deep recovery of hydrogen/deuterium in hydrogen/lithium deuteride as claimed in claim 5, wherein the mixture of the materials in step 4) is powdered or tableted.
10. The method for highly efficiently and deeply recovering hydrogen/deuterium from hydrogen/lithium deuteride as claimed in claim 5, wherein in the step 4), the content of hydrogen/lithium deuteride is 20-40 wt%.
11. The method as claimed in claim 5, wherein the reactor is heated to 400-610 ℃ in step 5).
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